CN109652798A - A kind of preparation method of Sintered NdFeB magnet surface composite coating - Google Patents
A kind of preparation method of Sintered NdFeB magnet surface composite coating Download PDFInfo
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- CN109652798A CN109652798A CN201910070014.3A CN201910070014A CN109652798A CN 109652798 A CN109652798 A CN 109652798A CN 201910070014 A CN201910070014 A CN 201910070014A CN 109652798 A CN109652798 A CN 109652798A
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- 239000011248 coating agent Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 51
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 13
- 238000005253 cladding Methods 0.000 claims abstract description 125
- 239000000463 material Substances 0.000 claims abstract description 79
- 229910052751 metal Inorganic materials 0.000 claims abstract description 72
- 239000002184 metal Substances 0.000 claims abstract description 72
- 239000000919 ceramic Substances 0.000 claims abstract description 69
- 239000000843 powder Substances 0.000 claims abstract description 58
- 239000000758 substrate Substances 0.000 claims abstract description 53
- 230000002787 reinforcement Effects 0.000 claims abstract description 37
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 22
- 239000000956 alloy Substances 0.000 claims abstract description 22
- 230000008018 melting Effects 0.000 claims abstract description 18
- 238000010309 melting process Methods 0.000 claims abstract description 10
- 238000002203 pretreatment Methods 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 33
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 21
- 229910052786 argon Inorganic materials 0.000 claims description 16
- 239000000835 fiber Substances 0.000 claims description 15
- 238000005554 pickling Methods 0.000 claims description 15
- 239000003921 oil Substances 0.000 claims description 14
- 230000001681 protective effect Effects 0.000 claims description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 10
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 10
- 238000005238 degreasing Methods 0.000 claims description 10
- 239000012530 fluid Substances 0.000 claims description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 8
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 8
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 238000005728 strengthening Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 238000007669 thermal treatment Methods 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 238000004506 ultrasonic cleaning Methods 0.000 claims 1
- 238000005299 abrasion Methods 0.000 abstract description 7
- 238000005260 corrosion Methods 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 13
- 239000000243 solution Substances 0.000 description 11
- 238000010907 mechanical stirring Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 239000011159 matrix material Substances 0.000 description 8
- 238000002844 melting Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000007921 spray Substances 0.000 description 7
- 238000009713 electroplating Methods 0.000 description 6
- 238000005507 spraying Methods 0.000 description 5
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 4
- 238000010411 cooking Methods 0.000 description 4
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- 230000008901 benefit Effects 0.000 description 3
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- 239000011253 protective coating Substances 0.000 description 3
- 239000012779 reinforcing material Substances 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
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- 238000007747 plating Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 229910000906 Bronze Inorganic materials 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- -1 silicon nitrides Chemical class 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a kind of preparation methods of Sintered NdFeB magnet surface composite coating, comprising the following steps: is uniformly mixed metal based alloys powder with metal based reinforcement material；The surface of using plasma melting and coating process, sintered NdFeB after the pre-treatment prepares Metal Substrate cladding layer；Ceramic based powders are uniformly mixed with ceramic based reinforcement material；Using plasma melting and coating process prepares ceramic base cladding layer on Metal Substrate cladding layer；Sintered NdFeB magnet after coating is heat-treated.The composite coating dense non-porous gap prepared through the invention has the characteristics that high-bond, high anti-corrosion, high abrasion, and more excellent corrosion protection effect can be provided for sintered NdFeB magnet.
Description
Technical field
The invention belongs to magnetic materials to protect field, and in particular to a kind of system of Sintered NdFeB magnet surface composite coating
Preparation Method.
Background technique
Sintered NdFeB magnet (NdFeB) is widely used with its excellent magnetic property (magnetic energy product, coercivity and remanent magnetism)
In the every field of national economy.Since Sintered NdFeB magnet mainly includes following three-phase: main phase Nd2Fe14B, rich-Nd phase and
Rich B phase, and the potential difference difference between each phase is larger, therefore is easily corroded in high temperature, humidity and electrochemical environment,
Seriously limit the further expansion of Sintered NdFeB magnet application field.In order to improve the corrosion resistance of Sintered NdFeB magnet
Can, generally use following two mode: addition alloying element method and surfacecti proteon facture.Wherein, alloying can be certain
The magnetic property of magnet is reduced in degree, and anticorrosion ability is unobvious.At present mainly using addition protective coating in industrial production
Mode improve the corrosion resistance of Sintered NdFeB magnet.
Currently, the common safeguard procedures in Sintered NdFeB magnet surface are as follows: plating, chemical plating, organic coating, physics gas
Mutually deposition and composite deposite.Wherein, electro-plating method is with simple to operation, cost input is low, is easily achieved mass production
Etc. advantages, be the most common technological means of neodymium iron boron magnetic body surfacecti proteon.But the protective coating table prepared using electro-plating method
Face binding force is low, and phenomena such as blistering, falling off easily occurs in coating, and coating porosity is high, and the discharge of electroplating wastewater easily causes ring
Border pollution problem.Magnet surface guard technology is proposed for the sophisticated technologies such as wind-power electricity generation, aerospace field higher
It is required that needing to develop the novel high-bond in Sintered NdFeB magnet surface, high anti-corrosion coating technology of preparing is one urgently to be resolved
Project.
Melting and coating technique includes laser melting and coating technique and plasma melting and coating technique.Its plasma cladding is developed recently
A kind of process for treating surface to get up, used plasma beam are a kind of ionization arcs.Compared with laser melting and coating technique, plasma
Body melting and coating technique is the plasma beam that high-temperature heating laser beam used is changed to high-energy density, is not likely to produce crackle, stomata
The defects of, technical process is simple, and pollution is few, and high production efficiency, raw material availability are high.The protection of plasma melting and coating technique preparation
It is metallurgical bonding between coating and matrix, there is very high binding force between coating and matrix.Directly in Sintered NdFeB magnet
Surface prepares ceramic base cladding layer and has the following problems: the matching between Sintered NdFeB magnet and ceramic base cladding layer is paid no attention to
Think, more hole is contained in coating, and brittleness is larger, causes the quality of ceramic base cladding layer not easy to control.
Summary of the invention
Based on this, the present invention provides a kind of preparation method of Sintered NdFeB magnet surface composite coating, including it is following
Step:
A kind of preparation method of Sintered NdFeB magnet surface composite coating, comprising the following steps:
A, the preparation of Metal Substrate cladding material: metal based alloys powder is uniformly mixed with metal based reinforcement material；
B, the preparation of Metal Substrate cladding layer: using plasma melting and coating process, the table of sintered NdFeB after the pre-treatment
Wheat flour is for Metal Substrate cladding layer；
C, the preparation of ceramic base cladding material: ceramic based powders are uniformly mixed with ceramic based reinforcement material；
D, the preparation of ceramic base cladding material: using plasma melting and coating process prepares ceramics on Metal Substrate cladding layer
Base cladding layer；
E, to through step d, treated that Sintered NdFeB magnet is heat-treated.
Further, in step a, the partial size of the metal based alloys powder is 20~200 μm, the Metal Substrate strengthening material
The partial size of material is 60~200nm；The mass ratio of the metal based alloys powder and metal based reinforcement material is (40~80): 1.
The alloy powder of different-grain diameter and metal based reinforcement material are mixed in the present invention, so as to improve the fiber morphology of coating, improved
The fiber stiffness of coating reduces the porosity of coating.While in order to further increase the performance of coating, it is preferred that by Metal Substrate
Alloy powder is as matrix phase, and using metal based reinforcement material as packing material, the preferably mass ratio of the two is (40~80): 1,
Coating performance can be made to be optimal.
Further, in step a, the metal based alloys powder is Co-based alloy powder, Co-based alloy powder, iron-based conjunction
The mixing at bronze end, one or more of acieral powder, the metal based reinforcement material be fibre reinforced materials,
The mixing of one or more of whisker reinforcement material, nano-particle reinforcement material.Here fibre reinforced materials can be with
Selected from carbon fiber, glass fibre etc., whisker reinforcement material and nano-particle reinforcement material can be selected from SiC, Si3N4、Al2O3·
B2O3, TiC etc., it is to be understood that the selection of the above material is only used for citing so that technical solution of the present invention is more clear
Chu, rather than limit the scope of protection of the present invention, the material selection that those skilled in the art know is used equally for the present invention
In.
Further, in step b, the parameter of the plasma melting and coating process are as follows: cladding electric current is 150~210A, is swept
Retouching speed is 2~12mm/s, and nozzle is 3~5g/min away from 4~10mm of magnet, powder sending quantity, and argon gas is as protective gas.
Further, in step b, the pretreatment successively includes oil removing, pickling and washing.
Preferably, for the degreasing fluid temperature that the oil removing uses for 55~95 DEG C, pH is 9~13, the oil removing time is 15~
25min；For the pickling solution that the pickling uses for the nitric acid solution of 10~24wt%, pickling time is 5~20s；The washing is
Ultrasound takes by storm 2~4min.
Further, in step c, the partial size of the ceramics based powders is 100~500 μm, the ceramics based reinforcement material
Partial size be 50~200nm；The mass ratio of the ceramics based powders and ceramic based reinforcement material is (30~60): 1.In the present invention
The ceramic based powders and ceramic based reinforcement material mixing for selecting different-grain diameter can improve the microstructure of coating, reduce hole
Rate improves microhardness.Specifically, using ceramic base alloy powder as matrix phase, ceramic based reinforcement material as packing material,
The mass ratio of the two is carried out preferably, preferably mass ratio (30~60): 1, so that coating performance of the invention reaches
It is optimal.Further, in step c, the ceramics based powders are the mixing of one or both of silicon nitride, silicon carbide, described
Ceramic based reinforcement material is the mixing of one or both of fibre reinforced materials, whisker reinforcement material.Due to silicon carbide and nitrogen
SiClx thermal conductivity is big, hardness is high, elevated temperature strength is big, inoxidizability is strong, wear resistance is good, thermal stability is good, thermal expansion coefficient is small,
Anti-thermal shock and resistant to chemical etching, therefore, preferably one of silicon nitride, silicon carbide is as ceramic based powders in the present invention.
Further, in step d, the parameter of the plasma melting and coating process are as follows: cladding electric current is 180~240A, is swept
Retouching speed is 3~10mm/s, and nozzle is 2~4g/min away from 4~10mm of magnet, powder sending quantity, and argon gas is as protective gas.
Further, which is characterized in that in step e, the process of thermal treatment parameter are as follows: 470~530 DEG C of temperature, when
Between 4~6h.
Compared with prior art, the invention has the following advantages: using plasma melting and coating technique of the present invention is pre-
NdFeB magnet surface that treated has been sequentially prepared Metal Substrate cladding layer and ceramic base cladding layer, while in Metal Substrate cladding layer
With reinforcing material, the thermal expansion coefficient of Metal Substrate cladding layer and NdFeB matrix are added in ceramic base cladding layer and ceramic base is molten
Coating has good matching, can form high bond strength with matrix and coating simultaneously, realize ceramic base cladding layer
With the best match between NdFeB matrix.Finally, being heat-treated to the neodymium iron boron magnetic body of coating composite coating, can eliminate
The stress generated between coating and matrix further increases film/film-substrate binding strength.Therefore, Metal Substrate/ceramic base of preparation is compound
Coating has an incomparable advantage of single cladding layer, the composite coating dense non-porous gap, have high-bond, it is high it is anti-corrosion,
The characteristics of high abrasion, can provide more excellent corrosion protection effect for sintered NdFeB magnet.
Specific embodiment
To facilitate the understanding of the present invention, below in conjunction with specific embodiments to invention is more fully described.But
It is that the invention can be realized in many different forms, however it is not limited to embodiments described herein.On the contrary, providing
The purpose of these embodiments is to make to make the present disclosure more fully understandable.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.
Embodiment 1
Specification is used (not magnetize, by Anhui the earth in the present embodiment for 24mm × 16mm × 3mm sintered NdFeB magnet
Bear new material limited liability company provides).
Magnet pretreatment: use temperature for 55 DEG C, pH value be 9 degreasing fluid to sintered NdFeB magnet oil removing 15min；So
The nitric acid solution pickling sintered NdFeB magnet 5s of 10wt% is used afterwards；Finally, magnet is cleaned by ultrasonic in deionized water
2min。
The preparation of Metal Substrate cladding material: by Co-based alloy powder (20 μm of partial size) and carbon fibre reinforcement, (partial size is
60nm) 40:1 is mixed in mass ratio, mechanical stirring 6h.
The preparation of Metal Substrate cladding layer: by pretreated sintered NdFeB magnet and prepared Metal Substrate cladding material
It is placed in plasma cladding equipment, prepares Metal Substrate cladding layer on sintered NdFeB magnet surface.The parameter of plasma cladding
Are as follows: cladding electric current is 150A, and scanning speed 2mm/s, nozzle is away from magnet 4mm, and powder sending quantity 3g/min, argon gas is as protection gas
Body.
The preparation of ceramic base cladding material: by silicon nitride ceramics based powders (100 μm of partial size) and carbon fibre reinforcement (grain
Diameter 50nm) 30:1 in mass ratio mixed, mechanical stirring 8h.
The preparation of ceramic base cladding layer: the sintered NdFeB magnet and ceramic base cladding material of Metal Substrate cladding layer will be coated
It is placed in plasma cladding equipment, prepares ceramic base cladding layer in the magnet surface of coating Metal Substrate cladding layer.Plasma
The condition of cladding are as follows: cladding electric current is 180A, and scanning speed 3mm/s, nozzle is away from magnet 4mm, powder sending quantity 2g/min, argon gas
As protective gas.
Magnet heat treatment: to the Sintered NdFeB magnet after coating composite coating in 470 DEG C of heat treatment 4h.By the present embodiment
Sample obtained is named as sample 1A.
Embodiment 2
Specification is used (not magnetize, by Anhui the earth in the present embodiment for 24mm × 16mm × 3mm sintered NdFeB magnet
Bear new material limited liability company provides).
Magnet pretreatment: use temperature for 75 DEG C, pH value be 10 degreasing fluid to sintered NdFeB magnet oil removing 20min；So
The nitric acid solution pickling sintered NdFeB magnet 12s of 17wt% is used afterwards；Finally, magnet is cleaned by ultrasonic in deionized water
3min。
The preparation of Metal Substrate cladding material: by Co-based alloy powder (110 μm of partial size) and carbon fibre reinforcement (partial size
130nm) 60:1 is mixed in mass ratio, mechanical stirring 8h.
The preparation of Metal Substrate cladding layer: by pretreated sintered NdFeB magnet and prepared Metal Substrate cladding material
It is placed in plasma cladding equipment, prepares Metal Substrate cladding layer on sintered NdFeB magnet surface.The parameter of plasma cladding
Are as follows: cladding electric current is 180A, and scanning speed 7mm/s, nozzle is away from magnet 7mm, and powder sending quantity 4g/min, argon gas is as protection gas
Body.
The preparation of ceramic base cladding material: by silicon nitride ceramics based powders (300 μm of partial size) and carbon fibre reinforcement (grain
Diameter 125nm) 45:1 in mass ratio mixed, mechanical stirring 10h.
The preparation of ceramic base cladding layer: the sintered NdFeB magnet and ceramic base cladding material of Metal Substrate cladding layer will be coated
It is placed in plasma cladding equipment, prepares ceramic base cladding layer in the magnet surface of coating Metal Substrate cladding layer.Plasma
The condition of cladding are as follows: cladding electric current is 180A, and scanning speed 3mm/s, nozzle is away from magnet 7mm, powder sending quantity 2g/min, argon gas
As protective gas.
Magnet heat treatment: to the Sintered NdFeB magnet after coating composite coating in 500 DEG C of heat treatment 5h.By the present embodiment
Sample obtained is named as sample 2A.
Embodiment 3
Specification is used (not magnetize, by Anhui the earth in the present embodiment for 24mm × 16mm × 3mm sintered NdFeB magnet
Bear new material limited liability company provides).
Magnet pretreatment: use temperature for 95 DEG C, pH value be 13 degreasing fluid to sintered NdFeB magnet oil removing 25min；So
The nitric acid solution pickling sintered NdFeB magnet 20s of 24wt% is used afterwards；Finally, magnet is cleaned by ultrasonic in deionized water
4min。
The preparation of Metal Substrate cladding material: by Co-based alloy powder (200 μm of partial size) and carbon fibre reinforcement (partial size
200nm) 80:1 is mixed in mass ratio, mechanical stirring 10h.
The preparation of Metal Substrate cladding layer: by pretreated sintered NdFeB magnet and prepared Metal Substrate cladding material
It is placed in plasma cladding equipment, prepares Metal Substrate cladding layer on sintered NdFeB magnet surface.The parameter of plasma cladding
Are as follows: cladding electric current is 210A, and scanning speed 12mm/s, nozzle is away from magnet 10mm, and powder sending quantity 5g/min, argon gas is as protection
Gas.
The preparation of ceramic base cladding material: by silicon nitride ceramics based powders (500 μm of partial size) and carbon fibre reinforcement (grain
Diameter 200nm) 60:1 in mass ratio mixed, mechanical stirring 12h.
The preparation of ceramic base cladding layer: the sintered NdFeB magnet and ceramic base cladding material of Metal Substrate cladding layer will be coated
It is placed in plasma cladding equipment, prepares ceramic base cladding layer in the magnet surface of coating Metal Substrate cladding layer.Plasma
The condition of cladding are as follows: cladding electric current is 240A, and scanning speed 10mm/s, nozzle is away from magnet 10mm, powder sending quantity 4g/min, argon
Gas is as protective gas.
Magnet heat treatment: to the Sintered NdFeB magnet after coating composite coating in 530 DEG C of heat treatment 6h.By the present embodiment
Sample obtained is named as sample 3A.
Embodiment 4
Specification is used (not magnetize, by Anhui the earth in the present embodiment for 24mm × 16mm × 3mm sintered NdFeB magnet
Bear new material limited liability company provides).
Magnet pretreatment: use temperature for 75 DEG C, pH value be 10 degreasing fluid to sintered NdFeB magnet oil removing 20min；So
The nitric acid solution pickling sintered NdFeB magnet 12s of 17wt% is used afterwards；Finally, magnet is cleaned by ultrasonic in deionized water
3min。
The preparation of Metal Substrate cladding material: by Co-based alloy powder (110 μm of partial size) and SiC reinforcing material (partial size
130nm) 60:1 is mixed in mass ratio, mechanical stirring 8h.
The preparation of Metal Substrate cladding layer: by pretreated sintered NdFeB magnet and prepared Metal Substrate cladding material
It is placed in plasma cladding equipment, prepares Metal Substrate cladding layer on sintered NdFeB magnet surface.The parameter of plasma cladding
Are as follows: cladding electric current is 180A, and scanning speed 7mm/s, nozzle is away from magnet 7mm, and powder sending quantity 4g/min, argon gas is as protection gas
Body.
The preparation of ceramic base cladding material: by silicon carbide ceramics based powders (300 μm of partial size) and alumina whisker strengthening material
Material (partial size 125nm) 45:1 in mass ratio is mixed, mechanical stirring 10h.
The preparation of ceramic base cladding layer: the sintered NdFeB magnet and ceramic base cladding material of Metal Substrate cladding layer will be coated
It is placed in plasma cladding equipment, prepares ceramic base cladding layer in the magnet surface of coating Metal Substrate cladding layer.Plasma
The condition of cladding are as follows: cladding electric current is 180A, and scanning speed 3mm/s, nozzle is away from magnet 7mm, powder sending quantity 2g/min, argon gas
As protective gas.
Magnet heat treatment: to the Sintered NdFeB magnet after coating composite coating in 500 DEG C of heat treatment 5h.
Embodiment 5
Specification is used (not magnetize, by Anhui the earth in the present embodiment for 24mm × 16mm × 3mm sintered NdFeB magnet
Bear new material limited liability company provides).
Magnet pretreatment: use temperature for 75 DEG C, pH value be 10 degreasing fluid to sintered NdFeB magnet oil removing 20min；So
The nitric acid solution pickling sintered NdFeB magnet 12s of 17wt% is used afterwards；Finally, magnet is cleaned by ultrasonic in deionized water
3min。
The preparation of Metal Substrate cladding material: by acieral powder (110 μm of partial size) and Si3N4Reinforcing material (partial size
130nm) 60:1 is mixed in mass ratio, mechanical stirring 8h.
The preparation of Metal Substrate cladding layer: by pretreated sintered NdFeB magnet and prepared Metal Substrate cladding material
It is placed in plasma cladding equipment, prepares Metal Substrate cladding layer on sintered NdFeB magnet surface.The parameter of plasma cladding
Are as follows: cladding electric current is 180A, and scanning speed 7mm/s, nozzle is away from magnet 7mm, and powder sending quantity 4g/min, argon gas is as protection gas
Body.
The preparation of ceramic base cladding material: by silicon carbide ceramics based powders (300 μm of partial size) and fiber glass reinforcement
(partial size 125nm) 45:1 in mass ratio is mixed, mechanical stirring 10h.
The preparation of ceramic base cladding layer: the sintered NdFeB magnet and ceramic base cladding material of Metal Substrate cladding layer will be coated
It is placed in plasma cladding equipment, prepares ceramic base cladding layer in the magnet surface of coating Metal Substrate cladding layer.Plasma
The condition of cladding are as follows: cladding electric current is 180A, and scanning speed 3mm/s, nozzle is away from magnet 7mm, powder sending quantity 2g/min, argon gas
As protective gas.
Magnet heat treatment: to the Sintered NdFeB magnet after coating composite coating in 500 DEG C of heat treatment 5h.
Comparative example 1
Specification is used (not magnetize, by Anhui the earth in this comparative example for 24mm × 16mm × 3mm sintered NdFeB magnet
Bear new material limited liability company provides).
Magnet pretreatment: use temperature for 95 DEG C, pH value be 9~13 degreasing fluid to sintered NdFeB magnet oil removing
25min；Then the nitric acid solution pickling sintered NdFeB magnet 20s of 24wt% is used；Finally, magnet is surpassed in deionized water
Sound cleans 4min.
The preparation of Zn is electroplated: using electro-deposition zinc coating on electroplating technology neodymium iron boron magnetic body surface after the pre-treatment, zinc
The electroplating technological parameter of coating: pH value 4.5, temperature are 30 DEG C, current density 2A/dm2, electroplating time 30min.It incite somebody to action this
Sample made from comparative example is named as sample 1B.
Comparative example 2
Specification is used (not magnetize, by Anhui the earth in this comparative example for 24mm × 16mm × 3mm sintered NdFeB magnet
Bear new material limited liability company provides).
Magnet pretreatment: use temperature for 95 DEG C, pH value be 9~13 degreasing fluid to sintered NdFeB magnet oil removing
25min；Then the nitric acid solution pickling sintered NdFeB magnet 20s of 24wt% is used；Finally, magnet is surpassed in deionized water
Sound cleans 4min.
The preparation of metal-based layer: using coating on spraying process neodymium iron boron magnetic body surface after the pre-treatment by 110 μ of partial size
The metal based coating of the carbon fibre reinforcement 60:1 in mass ratio composition of the cobalt-base alloys and partial size 130nm of m, spraying process is such as
Under: spraying fuel-flow control is 0.4MPa in 20mL/min, spray governor pressure, is atomized as 0.24MPa, the precuring 5min at 100 DEG C,
Subsequently into oven cooking cycle, oven cooking cycle temperature is 180 DEG C, baking time 30min.
The preparation of ceramic substrate: it is coated on the basis of metal-based layer using spraying process by 300 μm of silicon nitride potteries of partial size
The ceramic base coating of the carbon fibre reinforcement of porcelain based powders and partial size 125nm 45:1 in mass ratio composition, spraying process are as follows:
Fuel-flow control is sprayed in 25mL/min, spray governor pressure is 0.5MPa, is atomized as 0.26MPa, the precuring 4min at 120 DEG C, so
Enter oven cooking cycle afterwards, oven cooking cycle temperature is 2000 DEG C, baking time 40min.Sample made from this comparative example is named as
Sample 2B.
Comparative example 3
Specification is used (not magnetize, by Anhui the earth in this comparative example for 24mm × 16mm × 3mm sintered NdFeB magnet
Bear new material limited liability company provides).
Magnet pretreatment: use temperature for 95 DEG C, pH value be 9~13 degreasing fluid to sintered NdFeB magnet oil removing
25min；Then the nitric acid solution pickling sintered NdFeB magnet 20s of 24wt% is used；Finally, magnet is surpassed in deionized water
Sound cleans 4min.
The preparation of Metal Substrate cladding layer: by cobalt made of pretreated magnet and 200 μm of partial size of Co-based alloy powder
Base cladding material is placed in plasma cladding equipment, prepares cobalt-based cladding layer in NdFeB magnet surface.Plasma cladding
Parameter are as follows: cladding electric current is 210A, and scanning speed 12mm/s, nozzle is away from magnet 10mm, powder sending quantity 5g/min, argon gas conduct
Protective gas.
The preparation of ceramic base cladding layer: 500 μm of silicon nitrides of sintered NdFeB magnet and partial size of Metal Substrate cladding layer will be coated
Silicon nitride ceramic substrate cladding material made of ceramics is placed in plasma cladding equipment, in the magnet of coating Metal Substrate cladding layer
Surface prepares ceramic base cladding layer.The condition of plasma cladding are as follows: cladding electric current is 240A, scanning speed 10mm/s, spray
Mouth is away from magnet 10mm, and powder sending quantity 4g/min, argon gas is as protective gas.
Magnet heat treatment: to the Sintered NdFeB magnet after coating composite coating in 530 DEG C of heat treatment 6h.By the present embodiment
Sample obtained is named as sample 3B.
To sample 1B, 2B, the 3B prepared in sample 1A, 2A, the 3A and comparative example 1,2,3 prepared in embodiment 1,2,3 into
Row salt spray test [the condition of salt spray test are as follows: chamber temperature is 38 DEG C, and brine strength is 5% (volume ratio), using continuous spray
The test method of mist] and binding force test (national standard " sintered NdFeB overlay coating " GB/T 34491-2017), and it is wear-resisting to its
Property is tested (according to standard " the abrasion test method of the coat of metal " JIS H8503-1989), can be divided into according to abrasion loss
1 grade, 2 grades, 3 grades, 4 grades, 5 grades, rank is higher, and the abrasion loss that represents is bigger, and test result see the table below:
| Sample | Salt spray test (h) | Binding force (MPa) | Wearability (abrasion loss) |
| Sample 1A | 841 | 52 | 1 grade |
| Sample 2A | 840 | 53 | 1 grade |
| Sample 3A | 842 | 51 | 1 grade |
| Sample 1B | 72 | 7.52 | 4 grades |
| Sample 2B | 216 | 17.32 | 3 grades |
| Sample 3B | 192 | 51 | 3 grades |
As can be seen from the above table, the salt-fog resistant test ability of sample 1A, 2A, 3A is substantially better than the salt tolerant of sample 1B, 2B, 3B
Mist test capability, binding force is also apparently higher than sample 1B, 2B, and its abrasion loss is also significantly less than sample 1B, 2B, 3B, and explanation is adopted
Have with the coating ingredients after the cooperation optimization of plasma melting and coating technique in composite coating prepared by sintered NdFeB magnet surface and passes
The incomparable absolute predominance of system protective coating.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of preparation method of Sintered NdFeB magnet surface composite coating, which comprises the following steps:
A, the preparation of Metal Substrate cladding material: metal based alloys powder is uniformly mixed with metal based reinforcement material；
B, the preparation of Metal Substrate cladding layer: using plasma melting and coating process, the surface system of sintered NdFeB after the pre-treatment
Standby Metal Substrate cladding layer；
C, the preparation of ceramic base cladding material: ceramic based powders are uniformly mixed with ceramic based reinforcement material；
D, the preparation of ceramic base cladding material: it is molten to prepare ceramic base on Metal Substrate cladding layer for using plasma melting and coating process
Coating；
E, to through step d, treated that Sintered NdFeB magnet is heat-treated.
2. preparation method as described in claim 1, which is characterized in that in step a, the partial size of the metal based alloys powder is
20 ~ 200 μm, the partial size of the metal based reinforcement material is 60 ~ 200nm；The metal based alloys powder and Metal Substrate strengthening material
The mass ratio of material is (40 ~ 80): 1.
3. preparation method as claimed in claim 1 or 2, which is characterized in that in step a, the metal based alloys powder is cobalt
The mixing of one or more of base alloy powder, Co-based alloy powder, iron(-)base powder, acieral powder, institute
State metal based reinforcement material be one or both of fibre reinforced materials, whisker reinforcement material, nano-particle reinforcement material with
On mixing.
4. preparation method as described in claim 1, which is characterized in that in step b, the parameter of the plasma melting and coating process
Are as follows: cladding electric current is 150 ~ 210A, and scanning speed is 2 ~ 12mm/s, and for nozzle away from 4 ~ 10mm of magnet, powder sending quantity is 3 ~ 5g/min, argon
Gas is as protective gas.
5. preparation method as described in claim 1, which is characterized in that in step b, the pretreatment successively includes oil removing, acid
It washes and washes.
6. preparation method as claimed in claim 5, which is characterized in that the degreasing fluid temperature that the oil removing uses for 55 ~ 95 DEG C,
PH is 9 ~ 13, and the oil removing time is 15 ~ 25min；The pickling solution that the pickling uses is the nitric acid solution of 10 ~ 24wt%, pickling time
For 5 ~ 20s；The washing is 2 ~ 4min of ultrasonic cleaning.
7. preparation method as described in claim 1, which is characterized in that in step c, it is described ceramics based powders partial size be 100 ~
500 μm, the partial size of the ceramics based reinforcement material is 50 ~ 200nm；The quality of the ceramics based powders and ceramic based reinforcement material
Than for (30 ~ 60): 1.
8. preparation method as claimed in claim 1 or 7, which is characterized in that in step c, it is described ceramics based powders be silicon nitride,
The mixing of one or both of silicon carbide, the ceramics based reinforcement material are fibre reinforced materials, in whisker reinforcement material
One or two kinds of mixing.
9. preparation method as described in claim 1, which is characterized in that in step d, the parameter of the plasma melting and coating process
Are as follows: cladding electric current is 180 ~ 240A, and scanning speed is 3 ~ 10mm/s, and for nozzle away from 4 ~ 10mm of magnet, powder sending quantity is 2 ~ 4g/min, argon
Gas is as protective gas.
10. preparation method as described in claim 1, which is characterized in that in step e, the process of thermal treatment parameter are as follows: temperature
470 ~ 530 DEG C of degree, 4 ~ 6h of time.
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| EP3967407A1 (en) | 2020-09-07 | 2022-03-16 | Yantai Shougang Magnetic Materials Inc. | A preparation device and method of ceramic coating on a sintered type ndfeb permanent magnet |
| CN115101280A (en) * | 2022-07-26 | 2022-09-23 | 宁波大缙华磁性材料有限公司 | High-wear-resistance hydrogen-broken terbium neodymium iron boron magnet, preparation method thereof and cylindrical magnetic block made of neodymium iron boron magnet |
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